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NAMS 2002 Workshop - ICOM 2008

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Asymmetric Polymeric Membrane Formation – 4<br />

Tuesday July 15, 10:30 AM-11:00 AM, Wai’anae<br />

The Impact of Solvent on the Microstructure of Integrally Skinned<br />

Polyimide Nanofiltration Membranes before and after casting<br />

D. Patterson (Speaker), Department of Chemical and Materials Engineering, The University of<br />

Auckland, Auckland, New Zealand, darrell.patterson@auckland.ac.nz<br />

S. Costello, Department of Chemical and Materials Engineering, The University of Auckland,<br />

Auckland, New, Zealand<br />

A. Havill, Department of Chemical and Materials Engineering, The University of Auckland,<br />

Auckland, New, Zealand<br />

Y. See-Toh, Department of Chemical Engineering and Chemical Technology, Imperial College,<br />

London, UK<br />

A. Livingston, Department of Chemical Engineering and Chemical Technology, Imperial College,<br />

London, UK<br />

A. Turner, School of Biological Sciences, The University of Auckland, Auckland, New Zealand<br />

Due to their excellent resistance to a range of solvents, integrally skinned<br />

polyimide membranes have been used as nanofiltration membranes to achieve<br />

selective separations in a range of industrial and lab-scale chemical operations.<br />

These include: homogeneous catalyst recycle, petrochemical dewaxing, solvent<br />

exchange and chiral resolutions. However, despite the widening scope of use of<br />

these membranes, there is still little understanding of how different casting and<br />

filtration solvents affect their microstructure and how this impacts on membrane<br />

separation performance. Part of this question arises because the microstructure<br />

of nanofiltration membranes are typically characterised using dry membranes.<br />

However, during a filtration, the structure of the membrane changes when in<br />

contact with the solvent to be used, especially due to swelling. Therefore,<br />

although imaging a membrane outside of a solvent (dry) may give an indication<br />

of the initial microstructure prior to filtration, in order to understand how the<br />

microstructure affects the transport mechanism and thus membrane separation<br />

performance when it is being used, the membrane must be imaged when in<br />

solvent (wet).<br />

As a first step towards answering the above question, integrally skinned<br />

nanofiltration membranes were fabricated by phase inversion using Lenzing P84<br />

polyimide. A range of P84 membranes were fabricated, varying three formation<br />

parameters: doping solution solvents, evaporation time and post heat treatment<br />

temperature. The doping solvents used were n-methyl-2-pyrrolidone, dimethyl<br />

sulfoxide, dimethylformamide, 1,4-dioxane and acetone. The evaporation times<br />

varied were 10 seconds, 30 seconds and 60 seconds. The heat treatment<br />

temperatures were 100°C, 150°C and 200°C. The effect these parameters had<br />

on the membrane microstructure, filtration performance and mechanical strength<br />

were then characterised. The microstructure of these membranes, dry and in

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